CN1807471B - Vinyl acetate based high viscosity latex preparation method - Google Patents
Vinyl acetate based high viscosity latex preparation method Download PDFInfo
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- CN1807471B CN1807471B CN 200510031185 CN200510031185A CN1807471B CN 1807471 B CN1807471 B CN 1807471B CN 200510031185 CN200510031185 CN 200510031185 CN 200510031185 A CN200510031185 A CN 200510031185A CN 1807471 B CN1807471 B CN 1807471B
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Abstract
Basing on the Method for preparation of vinyl acetate heavy viscous latex, the reaction steps are: (1)adding sodium dodecylbenzene sulfonate 0. 2-0. 8 share, in aqueous solution of polyvinylalcohols 8-16 share, non-ionic surface active agent 2. 0-3. 5 share, water 50-90 share; (2) dripping vinyl acetate 70-105 share; (3) dripping 8-12% ammonium persulphate aqueous solution of 0. 1-0. 4 share, heating-up to 90-95deg C, cooling below 50deg C after reaction; (4)adding sodium carbonate aqueous solution, adjusting pH to 6; (5) adding dibutylphthalate, filtering discharge below 40 DEG C after agitate equably. The product of this invention is white homogeneous emulsion, its viscosity number is more than 7000mPa.S, pH 6, monomer residual value is less than 0. 5%, colloidal particle grain size is less than 0. 5mu m, this product is used to high-speed cigarette making machine, connector cigarette speed is more than 8000pay/min, hasing the characteristic of good early viscosity, high adhesive strength, smooth adhesion, good storing stabilization and so on.
Description
Technical field:
The invention belongs to the organic chemical industry, promptly based on the preparation method of vinyl acetate high-viscosity latex.
Background technology:
Vinyl acetate resin and modified resin latex thereof can be used for the bonding of aspects such as timber, paper, fabric, also can be used as main film forming matter, leather treatment, the cement modifier of building coating.Because such latex has advantage such as do not contain organic solvent, nontoxic, free from extraneous odour, tack is strong, adhering speed is fast, in a large number as cigarette glue, the viscosity of its cigarette glue generally is not more than 5000mPaS.In the last few years, China's cigarette industry used high-speed cigarette machine in a large number, and some super-huge cigar mill adopted special adhesion process, explicitly called for the viscosity of cigarette glue stick must be more than 7000mPaS.And as base-material---the latex of cigarette glue stick, its viscosity also must be more than 7000mPaS, otherwise, be difficult to satisfy the high speed cigarette manufacturing technique requirent.
Summary of the invention:
In order to improve the viscosity of cigarette glue, the invention provides a kind of satisfy viscosity greater than 7000mPaS, based on the preparation method of the high-viscosity latex of vinyl acetate, it can satisfy the special producing processing requirement of high speed cigarette, can satisfy the specification of quality of high-grade cigarette again.
Preparation method based on the vinyl acetate high-viscosity latex is characterized in that:
One, by weight proportion, contain following starting material:
1. vinyl acetate, colourless transparent liquid, 70～105 parts,
2. polyvinyl alcohol, white cotton-shaped powder, 8～16 parts,
3. Sodium dodecylbenzene sulfonate, white powder, 0.2～0.8 part,
4. nonionogenic tenside, white powder, 2.0～3.5 parts,
5. ammonium persulphate, white powder, 0.1～0.4 part,
6. dibutyl phthalate, colourless transparent liquid, 4.0～10 parts,
7. water, colourless liquid, 100～190 parts,
8. yellow soda ash, white powder, consumption is decided according to specific requirement;
Two, polyvinyl alcohol is put into reaction flask, add 50～100 parts in water, be warming up to 80～95 ℃, insulation, stirring until whole dissolvings, are cooled to 35～45 ℃ then, after the filtration, put into another reaction flask;
Three, ammonium persulphate being mixed with weight concentration is 8～12% the aqueous solution;
Four, polyreaction
1. in polyvinyl alcohol solution, add 50～90 parts of Sodium dodecylbenzene sulfonatees, nonionogenic tenside, water, stirred 20～30 minutes,
2. drip vinyl acetate,
3. drip ammonium persulfate solution, be warming up to 60 ℃～80 ℃, stir, be incubated 30～60 minutes, when not having obviously backflow, temperature is risen to 90～95 ℃, react after 20～30 minutes, be cooled to below 50 ℃,
4. add an amount of weight concentration and be 10～30% sodium carbonate solution, being adjusted to pH value is 6,
5. add dibutyl phthalate again, after stirring, filter discharging in 40 ℃ of following temperature.
When polyreaction, can add a kind of of following substances or several in the vinyl acetate, its weight ratio is:
1. butyl acrylate, colourless transparent liquid, 0～15 part,
2. vinylformic acid, colourless transparent liquid, 0～1.5 part,
3. methyl-propyl acid methyl esters, colourless transparent liquid, 0～5.0 part,
4. propenoic acid beta-hydroxy propyl ester, colourless transparent liquid, 0～7.0 part.
In order to make various substance reactions abundant, polyreaction can divide for two steps carried out:
One, seeding polymerization
1. in polyvinyl alcohol solution, add 50～90 parts of Sodium dodecylbenzene sulfonatees, nonionogenic tenside, water, stirred 20～30 minutes,
2. drip 10～20 parts of vinyl acetates,
3. drip ammonium persulfate solution, its dripping quantity is 30～40% of the ammonium persulfate solution total amount prepared, stirs 20～40 minutes, is warming up to 50 ℃～70 ℃;
Two, fully polymerization
1. after treating that the seeding polymerization reaction does not have obviously backflow, drip 60～85 parts of remaining vinyl acetates, 72～80 ℃ of control reaction temperature, and add remaining ammonium persulfate solution, divide and added for 8～12 times, stir, be incubated 30～60 minutes, when not having obviously backflow, temperature is risen to 90～95 ℃, react after 20～30 minutes, be cooled to below 50 ℃
2. add an amount of weight concentration and be 10～30% sodium carbonate solution, being adjusted to pH value is 6,
3. add dibutyl phthalate again, after stirring, filter discharging in 40 ℃ of following temperature.
When dividing two steps polymerizations, in abundant step of polymerization, can add a kind of in the following material or several in the remaining vinyl acetate, its weight ratio is:
1. butyl acrylate, colourless transparent liquid, 0～15 part,
2. vinylformic acid, colourless transparent liquid, 0～1.5 part,
3. methyl-propyl acid methyl esters, colourless transparent liquid, 0～5.0 part,
4. propenoic acid beta-hydroxy propyl ester, colourless transparent liquid, 0～7.0 part.
The kind of polyvinyl alcohol specifically can be: 1788,4.0～8.0 parts of polyvinyl alcohol, 1799,4.0～8.0 parts of polyvinyl alcohol.
The model of nonionogenic tenside can be OP-10.
Water in the starting material is preferably deionized water.
Product of the present invention is white homogeneous latex emulsion, and its viscosity number is greater than 7000mPaS, pH value 6, the monomer residue value is lower than 0.5%, the micelle granularity connects the mouth cigarette speed of a motor vehicle greater than 8000/minute less than 0.5 μ m, has that tack is good, bonding strength is high, bonding level and smooth, characteristics that shelf-stable is good.
Description of drawings
Fig. 1 is the process flow sheet of the embodiment of the invention 3.
Embodiment
Be described in detail as follows for 4 embodiment below:
Embodiment 1:
One, polyvinyl alcohol is put into reaction flask for 10 parts, add 65 parts in water, be warming up to 95 ℃, insulation, stirring until whole dissolvings, are cooled to 40 ℃ then, after the filtration, put into another reaction flask;
Two, with 0.15 part of aqueous solution that is mixed with weight concentration 10% of ammonium persulphate;
Three, polyreaction
1. in polyvinyl alcohol solution, add 0.3 part of Sodium dodecylbenzene sulfonate, 2.5 parts of nonionogenic tenside OP-10,60 parts in water, stirred 30 minutes;
2. drip 80 parts of vinyl acetates;
3. drip ammonium persulfate solution, be warming up to 70 ℃, stir, be incubated 50 minutes, when not having obviously backflow, temperature was risen to 95 ℃ of reactions after 30 minutes, be cooled to 40 ℃;
4. add an amount of weight concentration and be 15% sodium carbonate solution, regulating pH value is 6;
5. add 5 parts of dibutyl phthalates, after stirring, in the time of 30 ℃, filter discharging.
Embodiment 2:
In embodiment 1, when 2. the of polyreaction goes on foot, drip the mix monomer of 80 parts of vinyl acetates and following substances: 3 parts of butyl acrylates, 0.3 part in vinylformic acid, 2 parts of methyl-propyl acid methyl esters, 2 parts of propenoic acid beta-hydroxy propyl ester.
Embodiment 3:
One, with polyvinyl alcohol 1788,7.5 part, 1799,7.5 parts of polyvinyl alcohol, put into reaction flask, add 100 parts of swellings of deionized water 0.5 hour, be warming up to 80 ℃, stirred 4 hours, treat to be warming up to 95 ℃ after polyvinyl alcohol dissolves substantially, insulated and stirred is cooled to 40 ℃ then until whole dissolvings, puts after filtering in another reaction flask.
Two, it is standby 0.2 part of ammonium persulphate to be mixed with 10% the aqueous solution in burning the bosom.
Three, be placed with in the polyvinyl alcohol reaction flask of dissolution filter, add 0.3 part of Sodium dodecylbenzene sulfonate, nonionogenic tenside OP-10,2.8 parts, 60 parts of deionized waters, stir after 30 minutes, drip 15 parts of Vinyl Acetate Monomers, drip ammonium persulfate solution, its dripping quantity is 40% of the above-mentioned ammonium persulfate solution total amount of preparing, stirred 30 minutes, and be warming up to 60 ℃, carry out seeding polymerization.
Four, with 70 parts of remaining Vinyl Acetate Monomers with to put into minim pipette after 8.5 parts of propylene ester butyl esters, 1.0 parts in vinylformic acid, methyl methacrylate 3.5,5.0 parts of each monomers of propylene ester β-hydroxypropyl acrylate mix standby.
Five, after treating that seeding polymerization does not have obvious backflow, begin to drip the mix monomer of above-mentioned preparation, the control rate of addition, mix monomer was dripped off in 4 hours, 75 ℃ of control reaction temperature, and add one time ammonium persulfate solution every half an hour, its each additional amount by preparation ammonium persulfate solution total amount 7%, add 8 times, after treating that all monomer droppings are intact, stirred 10 minutes, add the residue ammonium persulfate solution, continued insulation reaction 30 minutes, when not having obviously backflow, temperature of reaction system is risen to 95 ℃, react after 25 minutes, be cooled to 40 ℃, the sodium carbonate solution that adds weight concentration 20%, regulating pH value is 6, adds 5 parts of dibutyl phthalates, after stirring, filter discharging in 30 ℃ of temperature and get final product.
Embodiment 4:
In embodiment 3, there is not the interpolation of butyl acrylate, vinylformic acid, methyl-propyl acid methyl esters, propenoic acid beta-hydroxy propyl ester in the step 4, in step 5, only drip 70 parts of vinyl acetates.
Claims (7)
1. based on the preparation method of vinyl acetate high-viscosity latex, it is characterized in that:
One, by weight proportion, contain following starting material:
1. vinyl acetate, colourless transparent liquid, 70～105 parts,
2. polyvinyl alcohol, white cotton-shaped powder, 8～16 parts,
3. Sodium dodecylbenzene sulfonate, white powder, 0.2～0.8 part,
4. nonionogenic tenside, white powder, 2.0～3.5 parts,
5. ammonium persulphate, white powder, 0.1～0.4 part,
6. dibutyl phthalate, colourless transparent liquid, 4.0～10 parts,
7. water, colourless liquid, 100～190 parts,
8. yellow soda ash, white powder, consumption is decided according to specific requirement;
Two, polyvinyl alcohol is put into reaction flask, add 50～100 parts in water, be warming up to 80～95 ℃, insulation, stirring until whole dissolvings, are cooled to 35～45 ℃ then, after the filtration, put into another reaction flask;
Three, ammonium persulphate being mixed with weight concentration is 8～12% the aqueous solution;
Four, polyreaction
1. in polyvinyl alcohol solution, add 50～90 parts of Sodium dodecylbenzene sulfonatees, nonionogenic tenside, water, stirred 20～30 minutes,
2. drip vinyl acetate,
3. drip ammonium persulfate solution, be warming up to 60 ℃～80 ℃, stir, be incubated 30～60 minutes, when not having obviously backflow, temperature is risen to 90～95 ℃, react after 20～30 minutes, be cooled to below 50 ℃,
4. add an amount of weight concentration and be 10～30% sodium carbonate solution, being adjusted to pH value is 6,
5. add dibutyl phthalate again, after stirring, filter discharging in 40 ℃ of following temperature, the viscosity number of gained vinyl acetate high-viscosity latex is greater than 7000mPaS.
2. the preparation method of high-viscosity latex according to claim 1 is characterized in that, when polyreaction, adds a kind of in the following material or several in the vinyl acetate, and its weight ratio is:
1. butyl acrylate, colourless transparent liquid, 0～15 part,
2. vinylformic acid, colourless transparent liquid, 0～1.5 part,
3. methyl-propyl acid methyl esters, colourless transparent liquid, 0～5.0 part,
4. propenoic acid beta-hydroxy propyl ester, colourless transparent liquid, 0～7.0 part.
3. based on the preparation method of vinyl acetate high-viscosity latex, it is characterized in that,
One, by weight proportion, contain following starting material:
1. vinyl acetate, colourless transparent liquid, 70～105 parts,
2. polyvinyl alcohol, white cotton-shaped powder, 8～16 parts,
3. Sodium dodecylbenzene sulfonate, white powder, 0.2～0.8 part,
4. nonionogenic tenside, white powder, 2.0～3.5 parts,
5. ammonium persulphate, white powder, 0.1～0.4 part,
6. dibutyl phthalate, colourless transparent liquid, 4.0～10 parts,
7. water, colourless liquid, 100～190 parts,
8. yellow soda ash, white powder, consumption is decided according to specific requirement;
Two, polyvinyl alcohol is put into reaction flask, add 50～100 parts in water, be warming up to 80～95 ℃, insulation, stirring until whole dissolvings, are cooled to 35～45 ℃ then, after the filtration, put into another reaction flask;
Three, ammonium persulphate being mixed with weight concentration is 8～12% the aqueous solution;
Four, polyreaction, divided for two steps carried out:
(1), seeding polymerization
1. in polyvinyl alcohol solution, add 50～90 parts of Sodium dodecylbenzene sulfonatees, nonionogenic tenside, water, stirred 20～30 minutes,
2. drip 10～20 parts of vinyl acetates,
3. drip ammonium persulfate solution, its dripping quantity is 30～40% of the ammonium persulfate solution total amount prepared, stirs 20～40 minutes, is warming up to 50 ℃～70 ℃;
(2), fully polymerization
1. after treating that the seeding polymerization reaction does not have obviously backflow, drip 60～85 parts of remaining vinyl acetates, 72～80 ℃ of control reaction temperature, and add remaining ammonium persulfate solution, divide and added for 8～12 times, stir, be incubated 30～60 minutes, when not having obviously backflow, temperature is risen to 90～95 ℃, react after 20～30 minutes, be cooled to below 50 ℃
2. add an amount of weight concentration and be 10～30% sodium carbonate solution, being adjusted to pH value is 6,
3. add dibutyl phthalate again, after stirring, filter discharging in 40 ℃ of following temperature, the viscosity number of gained vinyl acetate high-viscosity latex is greater than 7000mPaS.
4. the preparation method of high-viscosity latex according to claim 3 is characterized in that, in abundant step of polymerization, adds a kind of in the following substances or several in the remaining vinyl acetate, and its weight ratio is:
1. butyl acrylate, colourless transparent liquid, 0～15 part,
2. vinylformic acid, colourless transparent liquid, 0～1.5 part,
3. methyl-propyl acid methyl esters, colourless transparent liquid, 0～5.0 part,
4. propenoic acid beta-hydroxy propyl ester, colourless transparent liquid, 0～7.0 part.
5. the preparation method of high-viscosity latex according to claim 1 is characterized in that, the kind of polyvinyl alcohol is specially: 1788,4.0～8.0 parts of polyvinyl alcohol, 1799,4.0～8.0 parts of polyvinyl alcohol.
6. high-viscosity latex preparation method according to claim 1 is characterized in that the model of nonionogenic tenside is specially OP-10.
7. the preparation method of high-viscosity latex according to claim 1 is characterized in that, the water in the starting material is deionized water.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102181247B (en) * | 2011-03-22 | 2012-07-04 | 常德市金芙蓉精细化工有限责任公司 | Water-based superspeed cigarette lap adhesive and preparation method thereof |
| CN102229788B (en) * | 2011-05-13 | 2012-11-14 | 山西三维集团股份有限公司 | Preparation method for green and environment-friendly cigarette adhesive |
| CN102532371B (en) * | 2012-01-18 | 2013-10-16 | 重庆国际复合材料有限公司 | Preparation method of film-forming agent for glass fiber injection yarn |
| CN106008763A (en) * | 2016-06-28 | 2016-10-12 | 石媛 | Production method of polyvinyl acetate |
| CN107245315B (en) * | 2016-12-08 | 2018-03-20 | 中国科学院大连化学物理研究所 | A kind of formaldehydeless biomass-based environmental-protection type adhesive |
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